CN107219567A - A kind of uniform low-refraction optical filming material of film forming and preparation method - Google Patents

A kind of uniform low-refraction optical filming material of film forming and preparation method Download PDF

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Publication number
CN107219567A
CN107219567A CN201710476041.1A CN201710476041A CN107219567A CN 107219567 A CN107219567 A CN 107219567A CN 201710476041 A CN201710476041 A CN 201710476041A CN 107219567 A CN107219567 A CN 107219567A
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China
Prior art keywords
fluoride
filming material
low
optical filming
refraction
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CN201710476041.1A
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CN107219567B (en
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秦海波
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Beijing Fuxingkai Photo-Electronic Tech. Co., Ltd.
Huizhou Foryou Optical Technology Co., Ltd.
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Beijing Fuxingkai Photo-Electronic Tech Co Ltd
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    • GPHYSICS
    • G02OPTICS
    • G02BOPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B1/00Optical elements characterised by the material of which they are made; Optical coatings for optical elements
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0694Halides
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24Vacuum evaporation
    • GPHYSICS
    • G02OPTICS
    • G02BOPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B1/00Optical elements characterised by the material of which they are made; Optical coatings for optical elements
    • G02B1/10Optical coatings produced by application to, or surface treatment of, optical elements
    • G02B1/11Anti-reflection coatings
    • G02B1/113Anti-reflection coatings using inorganic layer materials only
    • G02B1/115Multilayers
    • GPHYSICS
    • G02OPTICS
    • G02BOPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B5/00Optical elements other than lenses
    • G02B5/08Mirrors

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  • Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Optics & Photonics (AREA)
  • General Physics & Mathematics (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Surface Treatment Of Optical Elements (AREA)
  • Optical Elements Other Than Lenses (AREA)
  • Physical Vapour Deposition (AREA)

Abstract

A kind of uniform low-refraction optical filming material of film forming and preparation method, belong to optical filming material technical field.Low-refraction optical filming material is made up of magnesium fluoride and additive calcirm-fluoride, barium fluoride or strontium fluoride, and the formula of low-refraction optical filming material is matched, mixed by weight, and through granulation, low-refraction optical filming material formulation by weight is as follows:Magnesium fluoride 80~99.5, the fluoride total amount 0.5~20 of addition;Carry out sintering for 3~6 hours more than 800 DEG C.During Coating Materials of the present invention is deposited on optical element, because simultaneously magnesium fluoride and calcirm-fluoride, barium fluoride, strontium fluoride etc. evaporate and are deposited on optical surface, because calcirm-fluoride, barium fluoride, strontium fluoride molecule effect, prevent the situation of oriented growth in original single magnesium fluoride deposition process, the evenly small optical film of stress is formed, due to the reduction of stress, when plating multilayer film, ensure the stabilization of multilayer film, the film for solving multilayer film splits problem.

Description

A kind of uniform low-refraction optical filming material of film forming and preparation method
Technical field
The present invention relates to a kind of uniform low-refraction optical filming material of film forming and preparation method, belong to optical coating material Expect technical field.
Background technology
In optical coating field, magnesium fluoride is a kind of conventional low-refraction optical filming material, because its refractive index is low, It is widely used in being coated with anti-reflection film, in film forming procedure, the process that magnesium fluoride is deposited on optical component surface is also in optics table The process of face recrystallization.Because the growth of crystal has certain directionality, process of such as water in icing, it will usually towards certain party To first growing, so, it will usually cause formed film microcosmic uneven, it is this it is microcosmic on it is uneven, plating multilayer film When can form stress, cause film to split.
The content of the invention
In order to overcome the deficiencies in the prior art, occurs the microcosmic inequality of film layer in special coating technique for magnesium fluoride material Even the problem of, the present invention provides a kind of uniform low-refraction optical filming material of film forming and preparation method.
A kind of preparation method of the uniform low-refraction optical filming material of film forming, low-refraction optical filming material, light Learn Coating Materials to be made up of magnesium fluoride and additive calcirm-fluoride, barium fluoride or strontium fluoride, contain following steps;
The formula of low-refraction optical filming material is matched, mixed by weight, through granulation,
Low-refraction optical filming material formula is following (weight proportion):
Magnesium fluoride 80~99.5%,
The fluoride total amount 0.5~20% of addition.
Carry out sintering for 3~6 hours more than 800 DEG C, or progress vacuum fusion 3~6 hours more than 1300 DEG C,
Carry out plated film:Plating conditions, coating machine diameter 1100mm, evaporation rate of the material in plated film is 10A0/ S, base 200 DEG C of glass sheet temperature.
A kind of uniform low-refraction optical filming material of film forming, formula is following (weight proportion):
Magnesium fluoride 80~99.5%,
The fluoride total amount 0.5~20% of addition;
By magnesium fluoride and calcirm-fluoride, barium fluoride, strontium fluoride etc., two or more mixture is constituted fluoride.
It is an advantage of the invention that in magnesium fluoride material, introducing a certain amount of other fluorides, such as calcirm-fluoride, barium fluoride fluorine Change strontium etc., so, during Coating Materials is deposited on optical element, due to magnesium fluoride and calcirm-fluoride, barium fluoride, strontium fluoride Deng evaporating simultaneously and be deposited on optical surface, because calcirm-fluoride, barium fluoride, strontium fluoride molecule effect, prevent original single fluorine Change the situation of oriented growth in magnesium deposition process, so, the small optical film of stress evenly can be formed, due to subtracting for stress It is small, when plating multilayer film, it is ensured that the stabilization of multilayer film, the film for solving multilayer film splits problem.
Embodiment
Obviously, those skilled in the art belong to the guarantor of the present invention based on many modifications and variations that spirit of the invention is done Protect scope.
Those skilled in the art of the present technique are appreciated that unless expressly stated, singulative " one " used herein, " one It is individual ", " described " and "the" may also comprise plural form.It is to be further understood that wording " the bag used in this specification Include " refer to there is the feature, integer, step, operation, element and/or component, but it is not excluded that in the presence of or addition one or Other multiple features, integer, step, operation, element, component and/or their group.It should be understood that when title element, component quilt When ' attach ' to another element, component, it, which can be directly connected to other elements, either component or can also have cental element Part or component.Wording "and/or" used herein includes one or more associated any cells for listing item and complete Combine in portion.
Those skilled in the art of the present technique are appreciated that unless otherwise defined, all terms used herein (including technology art Language and scientific terminology) with the general understanding identical meaning with the those of ordinary skill in art of the present invention.
For ease of the understanding to the embodiment of the present invention, explanation will be further explained below, and each embodiment is not Constitute the restriction to the embodiment of the present invention.
A kind of uniform low-refraction optical filming material of film forming, low-refraction optical filming material is by magnesium fluoride and fluorine Change two or more mixture such as calcium, barium fluoride, strontium fluoride composition.
Low-refraction optical filming material weight proportion is:Magnesium fluoride 80~99.5%, other fluoride fluorinating calcium, fluorinations Barium, strontium fluoride account for 0.5~20%.
Low-refraction optical filming material be magnesium fluoride and calcirm-fluoride, barium fluoride, strontium fluoride etc. two or more burning Tie mixture, the sintering temperature of the mixture is between 700 DEG C~1250 DEG C.
Low-refraction optical filming material can also be with magnesium fluoride and calcirm-fluoride, barium fluoride, strontium fluoride melting mixing Thing, the melting temperature of the molten mixture is more than 1300 DEG C.
The product produced using the low-refraction optical filming material.
900~1200 DEG C of the sintering temperature of low-refraction optical filming material.
Low-refraction optical filming material can be the molten mixture of several fluorides, fusion temperature 1300 DEG C with On.
Low-refraction optical filming material is used to plate reflective multilayer film.
Because calcirm-fluoride and barium fluoride, the refractive index of strontium fluoride are higher than the refractive index of magnesium fluoride, thus, calcirm-fluoride and fluorination Barium, strontium fluoride introduction volume can not be too high, otherwise can influence mixture refractive index, the amount of usually introducing is less than 20%.
The material component proportioning of 1~embodiment of embodiment 12 is shown in Table 1;
It is formulated each in table 1 by weight being matched, being mixed, through granulation, and more than 800 DEG C burn within 3~6 hours Knot, or vacuum fusion 3~6 hours is carried out more than 1300 DEG C, plated film experiment (plating conditions, plating are carried out to the product invented Film machine diameter 1100mm, evaporation rate of the material invented in plated film is 10A0/ S, 200 DEG C of base plate glass temperature)
(plated film tests 10A to the contrast experiment of table 10/S200℃)
By above-mentioned several groups of embodiments, by introducing a certain amount of calcirm-fluoride, barium fluoride, strontium fluoride in fluorination magnesium raw material Deng two or more mixture produce optical filming material, solve well because magnesium fluoride in coating process because The demoulding and film that the stress that crystallization, film forming are formed occurs split problem.
Finally it should be noted that:Obviously, above-described embodiment is only intended to clearly illustrate the application example, and simultaneously The non-restriction to embodiment.For those of ordinary skill in the field, it can also do on the basis of the above description Go out other various forms of changes or variation.There is no necessity and possibility to exhaust all the enbodiments.And thus drawn Among the obvious changes or variations that Shen goes out is still in the protection domain of the application.

Claims (9)

1. a kind of preparation method of the uniform low-refraction optical filming material of film forming, low-refraction optical filming material is by fluorine Change magnesium and additive calcirm-fluoride, barium fluoride or strontium fluoride composition, it is characterised in that contain following steps;
The formula of low-refraction optical filming material is matched, mixed by weight, through granulation,
Low-refraction optical filming material formulation by weight is as follows:
Magnesium fluoride 80~99.5,
The fluoride total amount 0.5~20 of addition;
Carry out sintering for 3~6 hours more than 800 DEG C.
2. a kind of preparation method of the uniform low-refraction optical filming material of film forming according to claim 1, its feature It is more than 1300 DEG C to carry out vacuum fusion 3~6 hours.
3. according to a kind of preparation method of the uniform low-refraction optical filming material of film forming described in claims 1 or 2, it is special Levy and be to carry out plated film:Plating conditions, coating machine diameter 1100mm, evaporation rate of the material in plated film is 10A °/S, substrate 200 DEG C of glass temperature.
4. a kind of uniform low-refraction optical filming material of film forming, is formulated following weight proportion:
Magnesium fluoride 80~99.5,
The fluoride total amount 0.5~20 of addition.
5. a kind of uniform low-refraction optical filming material of film forming according to claim 4, it is characterised in that fluoride By magnesium fluoride and calcirm-fluoride, barium fluoride, strontium fluoride etc., two or more mixture is constituted.
6. a kind of uniform low-refraction optical filming material of film forming according to claim 4, it is characterised in that low refraction Rate optical filming material is magnesium fluoride and calcirm-fluoride, barium fluoride, strontium fluoride two or more sintered mixture, sintered compound The sintering temperature of thing is between 700 DEG C~1250 DEG C.
7. a kind of uniform low-refraction optical filming material of film forming according to claim 4, it is characterised in that low refraction Rate optical filming material be also with magnesium fluoride and calcirm-fluoride, barium fluoride, strontium fluoride molten mixture, the melting of molten mixture Temperature is more than 1300 DEG C.
8. a kind of uniform low-refraction optical filming material of film forming according to claim 4, it is characterised in that low refraction 900~1200 DEG C of the sintering temperature of rate optical filming material.
9. a kind of uniform low-refraction optical filming material of film forming according to claim 4, it is characterised in that low refraction Rate optical filming material is used to plate reflective multilayer film.
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108254808A (en) * 2017-12-06 2018-07-06 惠州市华阳光学技术有限公司 A kind of optically functional film and preparation method thereof
CN109082632A (en) * 2018-08-20 2018-12-25 中国科学院上海技术物理研究所 A kind of infrared low-refraction the admixture plates the film material and preparation method
CN111733390A (en) * 2019-12-30 2020-10-02 宁波瑞凌新能源科技有限公司 Composite barrier material for double-reflection layer film and application thereof
CN111893433A (en) * 2020-07-30 2020-11-06 苏州瑞康真空科技有限公司 Coating material and preparation method thereof

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1505668A (en) * 2001-04-27 2004-06-16 �Ʒ� Multi-layered magnetic pigments and foils
CN101688292A (en) * 2007-06-28 2010-03-31 索尼株式会社 Low-refractive index film, method for forming the low-refractive index film, and antireflection film
US20110147676A1 (en) * 2009-12-22 2011-06-23 Sumitomo Metal Mining Co., Ltd. Oxide evaporation material and high-refractive-index transparent film
CN102324424A (en) * 2011-09-22 2012-01-18 华南师范大学 White-light LED (Light Emitting Diode) packaged by fluorescent transparent ceramic lens
CN205443429U (en) * 2015-12-24 2016-08-10 福建阭石创新材料股份有限公司 Preparation system of low refracting index evaporation coating materials

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1505668A (en) * 2001-04-27 2004-06-16 �Ʒ� Multi-layered magnetic pigments and foils
CN101688292A (en) * 2007-06-28 2010-03-31 索尼株式会社 Low-refractive index film, method for forming the low-refractive index film, and antireflection film
US20110147676A1 (en) * 2009-12-22 2011-06-23 Sumitomo Metal Mining Co., Ltd. Oxide evaporation material and high-refractive-index transparent film
CN102324424A (en) * 2011-09-22 2012-01-18 华南师范大学 White-light LED (Light Emitting Diode) packaged by fluorescent transparent ceramic lens
CN205443429U (en) * 2015-12-24 2016-08-10 福建阭石创新材料股份有限公司 Preparation system of low refracting index evaporation coating materials

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108254808A (en) * 2017-12-06 2018-07-06 惠州市华阳光学技术有限公司 A kind of optically functional film and preparation method thereof
CN109082632A (en) * 2018-08-20 2018-12-25 中国科学院上海技术物理研究所 A kind of infrared low-refraction the admixture plates the film material and preparation method
CN109082632B (en) * 2018-08-20 2021-01-01 中国科学院上海技术物理研究所 Infrared low-refractive-index mixed coating material and preparation method thereof
CN111733390A (en) * 2019-12-30 2020-10-02 宁波瑞凌新能源科技有限公司 Composite barrier material for double-reflection layer film and application thereof
CN111893433A (en) * 2020-07-30 2020-11-06 苏州瑞康真空科技有限公司 Coating material and preparation method thereof

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Inventor after: Qin Haibo

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Inventor after: Pan Shuo

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Address after: No. 14, Tianhe Road, Huangcun Town, Daxing District, Beijing

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Applicant after: Huizhou Foryou Optical Technology Co., Ltd.

Address before: No. 14, Tianhe Road, Huangcun Town, Daxing District, Beijing

Applicant before: Beijing Fuxingkai Photo-Electronic Tech. Co., Ltd.

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